SORPTION AND X-RAY FLUORESCENCE DETERMINATION OF MICRO QUANTITIES OF SOME TOXIC METALS IN NATURAL OBJECTS AFTER THEIR PRECONCENTRATION ON MODIFIED SILICA GEL

O. Kychkyruk, N. Kusiak, E. Yanovska
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Abstract

A method for X-ray fluorescence determination of trace amounts of Pb(II), Cd(II) and Hg(II) ions (up to 250 μg/ml) directly in the sorbent phase after their extraction from solutions  in a dynamic sorption mode has been developed. Merck silica gel (particle d 0.1-0.2 mm, specific surface 428.61 m2/g), chemically modified with 4-(2-pyridylazo)-resorcinol functional groups in one step, was used as a sorbent. An energy dispersive X-ray fluorescence analyzer with a semiconductor detector "ElvaX" ("Elvatex", Kyiv) was used in the study. It was found that the combined analysis of micro quantities of Pb, Cd and Hg by sorption-x-ray fluorescence method after their preconcentration on silica gel with chemically fixed  surfactant requires the use of calibration curves for each metal, taking into account the presence of other ions in solutions. The developed by us  method of  sorption-x-ray fluorescence  determination of  micro  quantities  of Pb(II), Cd(II) and Hg(II) after their extraction and preconcentration on silica gel with chemically fixed 4-(2-pyridylazo)-resorcinol can be effectively used for the analysis of natural and man-made objects of complex chemical composition.
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天然物体中某些有毒金属经改性硅胶预浓缩后的吸附和x射线荧光测定
建立了一种动态吸附模式下,在吸附相直接测定痕量Pb(II)、Cd(II)和Hg(II)离子(最高可达250 μg/ml)的方法。默克硅胶(粒径d 0.1 ~ 0.2 mm,比表面积428.61 m2/g)经4-(2-吡啶偶氮)间苯二酚官能团一步化学修饰,作为吸附剂。研究中使用了带有半导体探测器“ElvaX”(“Elvatex”,基辅)的能量色散x射线荧光分析仪。研究发现,用化学固定表面活性剂在硅胶上预富集微量铅、镉、汞后,用吸附-x射线荧光法联合分析微量铅、镉、汞,需要对每种金属使用校准曲线,同时考虑溶液中其他离子的存在。建立了用化学固定的4-(2-吡啶偶氮)间苯二酚在硅胶上萃取富集微量Pb(II)、Cd(II)和Hg(II)后的吸附-x射线荧光测定方法,可有效地用于化学成分复杂的天然和人造物体的分析。
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